TWI500632B - 高溫下的木質素分離方法 - Google Patents

高溫下的木質素分離方法 Download PDF

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TWI500632B
TWI500632B TW099122602A TW99122602A TWI500632B TW I500632 B TWI500632 B TW I500632B TW 099122602 A TW099122602 A TW 099122602A TW 99122602 A TW99122602 A TW 99122602A TW I500632 B TWI500632 B TW I500632B
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lignin
temperature
separation
heating
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Andrea Bonanni
Paolo Corbellani
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Beta Renewables Spa
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    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/06—Ethanol, i.e. non-beverage
    • C12P7/08—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate
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    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C1/00—Pretreatment of the finely-divided materials before digesting
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C1/00—Pretreatment of the finely-divided materials before digesting
    • D21C1/02—Pretreatment of the finely-divided materials before digesting with water or steam
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
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    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/003—Pulping cellulose-containing materials with organic compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • D21C3/024—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes with NH3 or H2O
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C7/00—Digesters
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Description

高溫下的木質素分離方法 發明背景
木質素的有效移除對得自生質的纖維素及糖類轉化成其它有機化合物諸如乙醇相當重要。
美國專利公告案200900381212 A1教示經由提升溶液溫度至高於臨界溫度，於該溫度木質素釋放水而自造紙廠液體去除木質素。該專利案進一步教示木質素團塊於處理程序期間加熱達分離之臨界溫度時，當團塊隨後冷卻時木質素固體沈澱，同時釋放出的水蓄積成上清液。
雖然此種方法可能可用於造紙廠液體，但於生質轉化的水解及發酵程序期間而變成自由態的木質素無法藉此方式分離。
 發明概要
本說明書揭示一種用以自水性混合物分離木質素之方法，包含下列步驟a)加熱該混合物至高於臨界溫度之溫度，及b)於分離溫度其係於或高於該臨界溫度，自該混合物分離該木質素。
該分離可透過離心、過濾、淘析、或其它可接受的技術包括重力進行。
進一步揭示混合物可含有將纖維素轉化成糖類之酶，混合物係衍生自生質進料，及/或於該加熱混合物步驟之前係對該生質進料進行蒸汽爆裂步驟。
進行分離之時間可於生質已經至少部分水解成糖類後，該至少部分水解的生質已經轉化成乙醇後，或自水分離乙醇之蒸餾步驟後。
進一步揭示混合物之pH為高於3.5或甚至高於7.0。
進一步揭示臨界溫度係於60℃至98℃之範圍，或溫度下限為70℃及溫度上限為97℃。
 較佳實施例之詳細說明
木質素為得自生質進料之產物生成後所留下的產物。舉例言之，於乙醇之製造中，生質進料通常於酶存在下，可首先經前處理，典型地係以蒸汽爆裂水解成糖類，然後糖類發酵而獲得乙醇。乙醇通常係藉蒸餾移除，留下水、木質素、酵母及其它酶。
自溶液分離木質素通常困難。咸信此係因木質素對水的高吸收性所致。US 20090038212宣稱經由首先自混合物分離木質素凝膠，加熱木質素至高於臨界溫度之溫度，然後冷卻木質素使得固體沈澱而不含水，可回收低含水液固體。
嘗試利用此種方法而自包含水、酵母及纖維素催化水解酶之水性混合物分離木質素業已失敗。冷卻時木質素並未沈澱，實際上，於高速離心後各相仍無法分離。
發現於木質素轉化成乙醇之處理程序期間所形成的水性混合物中之木質素，當混合物溫度係維持於或高於臨界溫度時可更有效地分離。
臨界溫度係關溶液之木質素的玻璃轉化溫度。相信一旦木質素加熱至高於其玻璃轉化溫度，釋放所吸收的水。玻璃轉化部分係取決於木質素類別、先前之熱處理(例如，水洗、蒸汽爆裂及水解)，及所吸收的水。
因此用於本說明書之目的，臨界溫度為木質素塑性固體釋放所吸收的水之溫度，相信該臨界溫度係約略為已經於先前條件下處理的該特定木質素之玻璃轉化溫度。雖然玻璃轉化溫度將改變，但臨界溫度係在下限低於已處理的木質素之玻璃轉化溫度起點10℃至上限為225℃界限的一定溫度範圍。225℃上限係由因大量水而被考慮為最高實用操作溫度之溫度決定。
更佳範圍為玻璃轉化溫度起點至97℃。觀察顯示超過某個溫度的更高溫度並未獲得更佳分離。實驗中，於80℃及90℃分離獲得極為類似的結果。基於目前已知，可接受的臨界溫度範圍為45℃至97℃、60℃至97℃、64℃至97℃、70℃至97℃、74℃至97℃、79℃至97℃、及84℃至97℃。
但若木質素已經以其它方式處理，則已知玻璃轉化溫度可能遽降。
雖然理論上並無混合物可被加熱的上限，但較佳混合物係加熱至高於臨界溫度但低於230℃，更佳係低於99℃。
加熱可藉專業人員期望的時間將混合物溫度升高至要求的溫度之任何方法施行。
木質素固體自混合物分離可藉任何技術進行，包括但非限於離心、重力沈積、過濾、淘析。
因該程序通常係於水解後進行，故混合物可含有至少一種可將纖維素轉成糖類之酶。多種酶為技藝界所已知，已明確確立酶是否能將纖維素轉成糖類之評估技術。
因混合物通常係衍生自生質進料，混合物加熱之前通常係對生質進料進行蒸汽爆裂步驟。生質特別為含纖維素之生質之蒸汽爆裂為技藝界眾所周知。
木質素之分離點可能出現在生質進料轉化期間的多點期間。舉例言之，混合物之加熱及分離可於生質已經至少部分水解成糖類之後，而於糖類發酵成終產物之前進行。
加熱及分離也可發生在該至少部分水解的生質已經轉成乙醇，也稱作為發酵步驟之後。
木質素之加熱及分離也可施行作為蒸餾步驟的一部分而自混合物之水分離乙醇。
pH也被視為有效參數，因此加熱及分離可於混合物之pH係高於7.0或至少高於3.5進行。
實驗
如下列實驗顯示，藉洗滌、蒸汽爆裂、水解及發酵而衍生自生質進料之混合物加熱至80℃，然後冷卻、加熱或維持溫度而於表I指示之溫度分離。樣本係於指示的溫度於3000 rpm離心歷經指示的時間。
該等樣本顯示有三相。第一相為液相，全部於80℃至95℃分離的樣本皆極為透明、琥珀色及清楚。於室溫標稱為23℃分離的樣本並未觀察得顯著相分離，實際上各相似乎略為顛倒，灰色固體狀材料係位在略微更深色的液相頂上。三相的出現於50℃，4分鐘至8分鐘的離心最明顯。
表I之測量值為沿試管壁之筆直部測得之材料總量高度測量時，含有目測可觀察相之試管百分比。該方法效率係以不含固體之液體量判定，對於80℃至95℃分離之材料約為80%。
減壓過濾
除了離心外，成功地減壓過濾也被呈現。
100毫升溶液係於0.5巴(bar)減壓下通過100平方厘米過濾面積過濾：其中該溶液係於25℃過濾之情況下，分離時間為190秒及乾燥時間為90秒。其中該溶液係於55℃過濾之情況下，分離時間為45秒及乾燥時間為15秒。
150毫升混合物係於0.5巴減壓下通過100平方厘米過濾面積過濾：其中該溶液係於25℃過濾之情況下，分離時間為420秒及乾燥時間為90秒。其中該溶液係於50℃過濾之情況下，分離時間為55秒及乾燥時間為15秒。
又藉由延長溫度，濾餅之終水分含量改良：於25℃之情況下濾餅水分為64.4%wt；而於55℃之情況下濾餅水分為59.16%wt。

Claims (12)

  1. 一種用以自具有pH高於3.5的水性混合物分離木質素之方法，其包含下列步驟：a)加熱該混合物至高於臨界溫度之溫度，該臨界溫度係於45℃至98℃之範圍，b)於分離溫度其係於或高於該臨界溫度，自該混合物分離該木質素固體，其中該混合物係衍生自生質進料及於該加熱混合物步驟之前係對該生質進料進行蒸汽爆裂步驟。
  2. 如申請專利範圍第1項之方法，其中該分離之至少部分係藉離心進行。
  3. 如申請專利範圍第1項之方法，其中該分離之至少部分係藉過濾進行。
  4. 如申請專利範圍第1項之方法，其中該分離之至少部分係藉重力進行。
  5. 如申請專利範圍第1項之方法，其中該混合物含有可將纖維素轉化成糖類之酶。
  6. 如申請專利範圍第5項之方法，其中該混合物之加熱係於該生質已經至少部分水解成糖類之後進行。
  7. 如申請專利範圍第6項之方法，其中該加熱混合物之步驟係於該至少部分水解的生質已經轉化成乙醇之後進行。
  8. 如申請專利範圍第1至7項中任一項之方法，其中該加 熱混合物步驟之一部分係進行作為蒸餾步驟的一部分，俾自水中分離乙醇。
  9. 如申請專利範圍第1至7項中任一項之方法，其中該混合物之pH係高於7.0。
  10. 如申請專利範圍第1至7項中任一項之方法，其中該臨界溫度係於具有溫度上限及溫度下限之範圍，及該溫度上限為97℃而該溫度下限為60℃。
  11. 如申請專利範圍第10項之方法，其中該溫度下限為70℃及該溫度上限為97℃。
  12. 如申請專利範圍第10項之方法，其中該溫度下限為74℃。
TW099122602A 2009-07-13 2010-07-09 高溫下的木質素分離方法 TWI500632B (zh)

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